WO2004086482A1 - Procede de nettoyage d'un appareil de formation de films minces - Google Patents

Procede de nettoyage d'un appareil de formation de films minces Download PDF

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Publication number
WO2004086482A1
WO2004086482A1 PCT/JP2004/004205 JP2004004205W WO2004086482A1 WO 2004086482 A1 WO2004086482 A1 WO 2004086482A1 JP 2004004205 W JP2004004205 W JP 2004004205W WO 2004086482 A1 WO2004086482 A1 WO 2004086482A1
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WO
WIPO (PCT)
Prior art keywords
thin film
nitrogen
reaction chamber
film forming
forming apparatus
Prior art date
Application number
PCT/JP2004/004205
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English (en)
Japanese (ja)
Inventor
Kazuhide Hasebe
Mitsuhiro Okada
Takashi Chiba
Jun Ogawa
Original Assignee
Tokyo Electron Limited
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Filing date
Publication date
Application filed by Tokyo Electron Limited filed Critical Tokyo Electron Limited
Priority to US10/549,851 priority Critical patent/US20060213539A1/en
Publication of WO2004086482A1 publication Critical patent/WO2004086482A1/fr

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
    • C23C16/4408—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber by purging residual gases from the reaction chamber or gas lines
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
    • C23C16/4404—Coatings or surface treatment on the inside of the reaction chamber or on parts thereof

Definitions

  • the present invention relates to a method for cleaning a thin film forming apparatus, and more particularly, to a method for cleaning a thin film forming apparatus for removing a reaction product attached to an exhaust system such as an exhaust pipe of the thin film forming apparatus.
  • a thin film is formed on an object to be processed, for example, a semiconductor wafer by a process such as CVD (Chemical Vapor Deposition).
  • CVD Chemical Vapor Deposition
  • a heat treatment apparatus as shown in FIG. 8 is used.
  • a reaction tube 52 having a double-tube structure composed of an inner tube 52 a and an outer tube 52 b is heated to a predetermined temperature, for example, 760 ° C. by heating 53.
  • a wafer boat 55 accommodating a plurality of semiconductor wafers 5 is loaded into the reaction tube 52 (inner tube 52 a).
  • the gas in the reaction tube 52 is exhausted from the exhaust port 56, and the pressure in the reaction tube 52 is reduced to a predetermined pressure, for example, 26.5 Pa (0.2 Torr).
  • the processing gas is supplied from the gas introduction tube 57 into the inner tube 52a.
  • the processing gas causes a thermal reaction, and a reaction product generated by the thermal reaction deposits on the surface of the semiconductor wafer 54, and the semiconductor wafer 5 A thin film is formed on the surface of 4.
  • Exhaust gas generated during the thin film forming process is exhausted to the outside of the heat treatment apparatus 51 via an exhaust port 56 and an exhaust pipe 58.
  • the exhaust pipe 58 is provided with a trap, a scrubber, and the like (not shown) so as to remove reaction products contained in the exhaust gas.
  • the reaction products generated during the thin film forming process are not only on the surface of the semiconductor wafer 54 but also on the inner surface of the heat treatment device 51 such as the inner wall of the inner tube 52 a. It accumulates (adheres). If the thin film forming process is continued with the reaction products attached to these members, the reaction products will eventually peel off and generate particles. These particles can adhere to the semiconductor wafer 54 and reduce the yield of the manufactured semiconductor device.
  • the thin film forming process is performed as many times as no particles are generated.
  • the inside of the heat treatment apparatus 51 is heated to a predetermined temperature by the heater 53, and a mixed gas of fluorine and a halogen-containing acid gas (cleaning gas, for example) is introduced into the heated heat treatment apparatus 51.
  • a mixed gas of fluorine and a halogen-containing acid gas cleaning gas, for example
  • the fluorine contained in the cleaning gas diffuses into the material in the reaction tube 52, for example, quartz. Then, even if nitrogen gas is supplied into the heat treatment apparatus 51, the fluorine is hardly discharged out of the heat treatment apparatus 51.
  • the thin film forming process is performed in a state where fluorine is diffused in the quartz constituting the reaction tube 52, fluorine is diffused (outwardly diffused) from the reaction tube 52 during the thin film forming process. obtain. In this case, the fluorine concentration in the thin film formed on the semiconductor wafer 54 increases.
  • the conventional heat treatment apparatus 51 repeatedly performs a thin film forming process for depositing a reaction product on the surface of the semiconductor wafer 54 in the reaction tube 52 maintained at a high temperature and a low pressure. For this reason, even if the inside of the apparatus is periodically cleaned, a small amount of impurities may be released (generated) from quartz, which is a material forming the reaction tube 52.
  • quartz which is a material constituting the reaction tube 52, contains a trace amount of metal contaminants (metal contamination) made of copper or the like, and this metal contamination is generated from the reaction tube 52 during the thin film forming process. Can diffuse outward. If impurities such as metal contaminants adhere to the semiconductor wafer 54, the yield of the manufactured semiconductor device will decrease.
  • the present invention has been made in view of the above problems, and an object of the present invention is to provide a thin film forming apparatus, a method of cleaning the thin film forming apparatus, and a method of forming a thin film, which can suppress the entry of impurities into a formed thin film.
  • Another object of the present invention is to provide a thin film forming apparatus, a method of cleaning the thin film forming apparatus, and a method of forming a thin film that can suppress diffusion of impurities such as fluorine and metal contaminants during the thin film forming process. .
  • Still another object of the present invention is to provide a thin film forming apparatus, a method of cleaning the thin film forming apparatus, and a method of forming a thin film that can suppress the concentration of impurities such as fluorine and metal contaminants in a formed thin film at a low level.
  • a method for cleaning a thin film forming apparatus is a method for cleaning a thin film forming apparatus for forming a thin film on a target object by supplying a processing gas into a reaction chamber accommodating the target object.
  • the surfaces of members in the reaction chamber are nitrided by the activated nitrogen-based gas. For this reason, it becomes difficult for impurities to be released from the members in the reaction chamber, and the contamination of the thin film with impurities can be suppressed.
  • the present invention provides a method for cleaning a thin film forming apparatus for forming a thin film on a target object by supplying a processing gas into a reaction chamber accommodating the target object, wherein the activation includes nitrogen in the reaction chamber.
  • the activated nitrogen-based gas reacts with a metal contaminant contained in a member in the reaction chamber, for example, a member constituting the reaction chamber, thereby removing the metal contaminant from the member. .
  • a metal contaminant contained in a member in the reaction chamber for example, a member constituting the reaction chamber, thereby removing the metal contaminant from the member.
  • the amount of metal contaminants contained in the members in the reaction chamber is low.
  • the diffusion of metal contaminants during thin film formation is suppressed. Therefore, the concentration of metal contaminants in the formed thin film is reduced.
  • impurities are less likely to be mixed into the thin film.
  • the present invention is a method for cleaning a thin film forming apparatus for forming a thin film on a target object by supplying a processing gas into a reaction chamber accommodating the target object, wherein the cleaning gas contains fluorine in the reaction chamber.
  • the purging step activates the nitrogen-based gas, and reacts the fluorine-based gas diffused into the members in the reaction chamber with the activated nitrogen-based gas in the adhering matter removing step.
  • the method for cleaning a thin film forming apparatus further comprises the step of removing the fluorine from the member.
  • the activated nitrogen-based gas reacts with fluorine diffused in a member in the reaction chamber, for example, a member constituting the reaction chamber, and fluorine is removed from the member.
  • fluorine diffused in a member in the reaction chamber for example, a member constituting the reaction chamber
  • fluorine concentration in the formed thin film is reduced.
  • impurities are less likely to be mixed into the thin film.
  • the present invention is a method for cleaning a thin film forming apparatus for forming a thin film on a processing object by supplying a processing gas into a reaction chamber accommodating the processing object, wherein the cleaning chamber contains fluorine.
  • a purging step wherein the purging step includes a step of activating the nitrogen-based gas to nitride a surface of a member in the reaction chamber. This is a cleaning method.
  • the surface of a member in the reaction chamber is nitrided by the activated nitrogen-based gas.
  • the nitrogen-based gas is, for example, ammonia, nitrous oxide, or nitric oxide.
  • the inside of the reaction chamber is maintained at 133 Pa to 53.3 kPa.
  • the nitrogen-based gas is activated by being supplied into the reaction chamber heated to a predetermined temperature.
  • the temperature of the reaction chamber is raised to 600 ° C .;
  • the members in the reaction chamber are made of quartz.
  • the processing gas includes ammonia and a gas containing silicon
  • the thin film is a silicon nitride film
  • the nitrogen-based gas is ammonia.
  • the gas containing silicon is dichlorosilane, hexachlorodisilane, monosilane, disilane, tetrachlorosilane, trichlorosilane, bisbutyl butylaminosilane, or hexethylaminodisilane.
  • the present invention provides a cleaning step of cleaning the thin film forming apparatus according to the method of cleaning a thin film forming apparatus having any one of the above characteristics, and increasing a temperature of a reaction chamber accommodating an object to be processed to a predetermined temperature; A film forming step of supplying a processing gas into the reaction chamber to form a thin film on the object to be processed.
  • ADVANTAGE OF THE INVENTION According to this invention, it becomes difficult to discharge
  • the present invention is a thin film forming apparatus for forming a thin film on a processing object by supplying a processing gas into a reaction chamber accommodating the processing object, wherein activatable nitrogen containing nitrogen is contained in the reaction chamber.
  • a nitrogen-based gas supply unit for supplying a system gas; an activation unit for activating the nitrogen-based gas; and controlling the activation unit to activate the nitrogen-based gas.
  • a nitriding means for nitriding the surface.
  • the surface of the member in the reaction chamber is nitrided by the nitrogen-based gas activated by the activation means. For this reason, impurities are less likely to be released from members in the reaction chamber, and contamination of the thin film with the impurities can be suppressed.
  • the processing gas is supplied to a reaction chamber for accommodating the object to be processed
  • a thin film forming apparatus for forming a thin film on an object to be processed, comprising: a nitrogen-based gas supply unit configured to supply an activatable nitrogen-based gas including nitrogen into the reaction chamber; and an activation unit configured to activate the nitrogen-based gas.
  • Means for activating the nitrogen-based gas by controlling the activating means, and reacting the activated metal-based gas with a metal contaminant contained in a member in the reaction chamber.
  • a contaminant removal control means for removing contaminants from the member.
  • the nitrogen-based gas activated by the activating means reacts with the metal contaminant contained in the member in the reaction chamber, and the metal contaminant is removed from the member. For this reason, the amount of metal contaminants contained in the members in the reaction chamber is reduced, and the diffusion of metal contaminants during thin film formation is suppressed. Therefore, the concentration of metal contaminants in the formed thin film is reduced. Further, impurities are less likely to be mixed into the thin film.
  • the present invention is a thin film forming apparatus that supplies a processing gas into a reaction chamber accommodating an object to be processed and forms a thin film on the object to be processed, wherein a cleaning gas that supplies a cleaning gas containing fluorine into the reaction chamber is provided.
  • a gas supply unit a nitrogen-based gas supply unit that supplies an activatable nitrogen-based gas containing nitrogen into the reaction chamber, an activation unit that activates the nitrogen-based gas, and a control unit that controls the activation unit.
  • Activating the nitrogen-based gas to cause the fluorine diffused in the member in the reaction chamber to react with the activated nitrogen-based gas, thereby removing the fluorine from the member.
  • the nitrogen-based gas activated by the activating means reacts with the fluorine diffused into the member in the reaction chamber, and fluorine is removed from the member. For this reason, the amount of fluorine diffused into the members in the reaction chamber is reduced, and the diffusion of fluorine during the formation of the thin film is suppressed. Therefore, the concentration of fluorine in the formed thin film is reduced. Furthermore, impurities are less likely to be mixed into the thin film.
  • the present invention is a thin film forming apparatus that supplies a processing gas into a reaction chamber accommodating an object to be processed and forms a thin film on the object to be processed, wherein a cleaning gas that supplies a cleaning gas containing fluorine into the reaction chamber is provided.
  • a gas supply unit a nitrogen-based gas supply unit that supplies an activatable nitrogen-based gas containing nitrogen into the reaction chamber, an activation unit that activates the nitrogen-based gas, and a control unit that controls the activation unit.
  • a nitriding means for nitriding the surface of the member in the reaction chamber.
  • the surface of the member in the reaction chamber is nitrided by the nitrogen-based gas activated by the activation means. This makes it difficult for fluorine in the members in the reaction chamber to diffuse (release), and suppresses the diffusion of fluorine during thin film formation. Therefore, the concentration of fluorine in the formed thin film is reduced. Further, the contamination of the thin film with impurities can be suppressed.
  • the nitrogen-based gas is, for example, ammonia, nitrous oxide, or nitric oxide.
  • the activating means is, for example, a heating means.
  • the activating means is a plasma generating means.
  • the activating means is a photolytic means.
  • the activating means is a catalyst activating means.
  • the activating means is means for raising the temperature of the reaction chamber to 600 ° C. to 150 ° C.
  • the thin film forming apparatus further includes pressure adjusting means for maintaining the pressure in the reaction chamber at 13 to 53.3 kPa.
  • FIG. 1 is a diagram showing a thin film forming apparatus according to one embodiment of the present invention.
  • FIG. 2 is a diagram showing a recipe for explaining a thin film forming method according to one embodiment of the present invention.
  • FIG. 3 is a diagram showing a recipe for explaining a thin film forming method according to another embodiment of the present invention.
  • FIG. 4 is a graph showing the relationship between the depth of the quartz chip and the fluorine concentration.
  • FIG. 5 is a graph showing the relationship between the depth of the quartz chip and the secondary ion intensity of nitrogen.
  • FIG. 6 is a graph showing the relationship between the purge gas and the copper concentration.
  • FIG. 7 is a diagram showing a thin film forming apparatus according to another embodiment of the present invention.
  • FIG. 8 is a diagram showing a conventional thin film forming apparatus. BEST MODE FOR CARRYING OUT THE INVENTION
  • the heat treatment apparatus 1 includes a substantially cylindrical reaction tube 2 whose longitudinal direction is directed vertically.
  • the reaction tube 2 has a double tube structure composed of an inner tube 3 and an outer tube 4 having a ceiling and formed so as to cover the inner tube 3 and to have a certain distance from the inner tube 3.
  • the inner tube 3 and the outer tube 4 are formed of a heat-resistant material, for example, quartz.
  • a manifold 5 made of stainless steel (SUS) formed in a cylindrical shape is arranged below the outer tube 4.
  • the manifold 5 is air-tightly connected to the lower end of the outer tube 4.
  • the inner pipe 3 is supported by a support ring 6 formed to protrude from the inner wall of the manifold 5.
  • a lid 7 is disposed below the manifold 5.
  • the lid 7 is configured to be able to move up and down by the boat elevator 8. When the lid 7 is raised by the boat elevator 8, the lower side of the manifold 5 is closed.
  • a wafer boat 9 made of, for example, quartz is placed on the lid 7.
  • the wafer boat 9 can accommodate a plurality of objects to be processed, for example, semiconductor wafers 10 at predetermined intervals in the vertical direction.
  • a heat insulator 11 is provided around the reaction tube 2 so as to surround the reaction tube 2.
  • a heating heater 12 made of a resistance heating element is provided on the inner wall surface of the heat insulator 11.
  • the temperature of the inside of the reaction tube 2 is increased to a predetermined temperature by the heating heater 12, and as a result, the semiconductor device 10 is heated to the predetermined temperature.
  • a plurality of processing gas introduction pipes 13 for introducing a processing gas are passed through a side surface of the manifold 5. In FIG. 1, only one processing gas introduction pipe 13 is shown.
  • the processing gas introduction pipe 13 is passed below the support ring 6 so as to face the inner pipe 3.
  • the processing gas introduction pipe 13 is connected to a predetermined processing gas supply source (not shown) via a mass flow controller (not shown) or the like.
  • Silicon on semiconductor wafer 10 When a nitride film (SiN film) is formed, it is connected to, for example, an ammonia (NH 3 ) gas supply source and a gas supply source containing silicon.
  • NH 3 ammonia
  • Gas containing silicon For example, dichlorosilane (S i H 2 C 12: DCS), the hexa-chloro disilane (S i 2 C 1 ⁇ ) , monosilane (S i H 4), disilane (S i 2 H 6 ), tetrachloroethene port silane (S i C l 4), trichlorosilane (S i HC ls), bis evening one charb chill aminosilane, to hexa E chill aminodisilanes.
  • DCS gas supply source for this reason, a predetermined amount of ammonia gas and DCS gas are introduced into the inner pipe 3 from the processing gas introduction pipe 13.
  • FIG. 1 shows only one cleaning gas introduction pipe 14.
  • the cleaning gas introduction pipe 14 is disposed so as to face the inside of the inner pipe 3, and the cleaning gas is introduced from the cleaning gas introduction pipe 14 into the inner pipe 3.
  • the cleaning gas introduction pipe 14 is connected to a predetermined cleaning gas supply source (not shown), for example, a fluorine gas supply source, a hydrogen fluoride gas supply source, and a nitrogen gas supply source via a mask port controller (not shown). Has been done.
  • a nitrogen-based gas introduction pipe 15 for introducing a nitrogen-based gas is provided on a side surface of the manifold 5.
  • the nitrogen-based gas may be any gas containing nitrogen and capable of being excited (activated), such as ammonia, nitrous oxide (N 20 ), and nitric oxide (NO). With this nitrogen-based gas, it is possible to nitride a member inside the heat treatment apparatus 1, for example, a member made of stone.
  • the nitrogen-based gas introduction pipe 15 is arranged so as to face the inside of the inner pipe 3.
  • the nitrogen-based gas introduction pipe 15 is connected to a gas supply source (not shown) via a mass flow controller (not shown). Therefore, the nitrogen-based gas is introduced into the inner pipe 3 from a gas supply source (not shown) via the nitrogen-based gas introduction pipe 15.
  • a discharge port 16 is also provided on the side of the manifold 5.
  • the discharge port 16 is provided above the support ring 6 and communicates with a space formed between the inner tube 3 and the outer tube 4 in the reaction tube 2. Then, exhaust gas or the like generated in the inner pipe 3 passes through the space between the inner pipe 3 and the outer pipe 4 and is exhausted to the exhaust port 16.
  • a purge gas supply pipe 17 for supplying nitrogen gas as a purge gas is passed.
  • An exhaust pipe 18 is hermetically connected to the outlet 16.
  • the exhaust pipe 18 is provided with a valve 19 and a vacuum pump 20 from the upstream side.
  • the valve 19 adjusts the opening of the exhaust pipe 18 to control the pressure in the reaction pipe 2 to a predetermined pressure.
  • the vacuum pump 20 exhausts the gas inside the reaction tube 2 via the exhaust tube 18 and adjusts the pressure inside the reaction tube 2.
  • a trap (not shown) and a scrubber (not shown) are provided in the exhaust pipe 18.
  • the exhaust gas exhausted from the reaction pipe 2 is detoxified and then exhausted outside the heat treatment apparatus 1. ing.
  • the control unit 21 is connected to the vacuum pump 20.
  • the control unit 21 includes a microprocessor, a process controller, and the like, measures the temperature, pressure, and the like of each unit of the heat treatment apparatus 1, outputs a control signal and the like to each of the above units based on the measurement data, and Each part of 1 is controlled according to the recipe (time sequence) shown in Fig. 2 or Fig. 3.
  • a thin film forming method including a purging process as a cleaning method of the heat treatment apparatus 1 and a film forming process of forming a silicon nitride film on the semiconductor wafer 10 will be described with reference to the recipe in FIG. .
  • the temperature of the inside of the reaction tube 2 is raised to a predetermined load temperature, that is, 300 ° C. as shown in FIG. As shown in FIG. 2 (c), after a predetermined amount of nitrogen gas is supplied from the purge gas supply pipe 17 into the reaction pipe 2, the wafer boat 9 containing no semiconductor wafer 10 is covered. Place on body 7. And bo — Raise the lid 7 with the lid 8 and seal the reaction tube 2 (loading process). Next, the gas in the reaction tube 2 is discharged, and the inside of the reaction tube 2 is set to a predetermined pressure.
  • the pressure in the reaction tube 2 is preferably set to 133 Pa (l. 0 Torr) to 53.3 kPa (400 Torr).
  • the pressure in the reaction tube 2 is set to 2660 Pa (20 Torr) to 53.3 kPa (400 Torr).
  • the pressure is set to 2660 Pa (20 Torr).
  • the inside of the reaction tube 2 is heated to a predetermined temperature by the heating heater 12. It is preferable that the temperature in the reaction tube 2 be set to 600 ° C to 1050 ° C. If the temperature is lower than 600 ° C., in the ammonia purging step, outward diffusion of impurities (metal contamination, fluorine, etc.) in the quartz constituting the reaction tube 2 and nitridation of the quartz constituting the reaction tube 2 are performed. It may be difficult. On the other hand, if the temperature is higher than 1050 ° C., the temperature exceeds the softening point of the quartz constituting the reaction tube 2. More preferably, the temperature inside the reaction tube 2 is set to 800 ° C to 1050 ° C. When the temperature is 800 ° C.
  • the temperature is increased to 900 ° C. as shown in FIG.
  • stabilization step When the inside of the reaction tube 2 is stabilized at a predetermined pressure and temperature, a predetermined amount of nitrogen-based gas, for example, ammonia gas as shown in FIG. Little / min supplied.
  • the vacuum pump 20 is driven while the opening of the valve 19 is controlled, and the gas in the reaction tube 2 is discharged. Then, the supply of the ammonia gas and the discharge of the gas in the reaction tube 2 are repeated a plurality of times (ammonia purge step).
  • the quartz constituting the reaction tube 2 and the like contains impurities, for example, metal contaminants (metal contamination). Impurities mixed into the quartz constituting the reaction tube 2 etc. It is difficult to process the reaction tube 2 so that it does not occur.
  • metal such as copper is contained in quartz depending on the contents of the processing step of the reaction tube 2 and the like and the working atmosphere.
  • the ammonia gas is supplied into the inner tube 3
  • the ammonia in the reaction tube 2 is excited (activated) by the heat in the reaction tube 2 and reacts with the metal contamination contained in the quartz constituting the reaction tube 2.
  • metal contamination is diffused (outwardly diffused) from the quartz constituting the reaction tube 2 and becomes chewy.
  • the amount of metal contaminants contained in the quartz constituting the reaction tube 2 is reduced, and the diffusion of the metal contaminants from the reaction tube 2 during the film forming process can be reduced. As a result, the amount (concentration) of metal contamination in the silicon nitride film formed by the film forming process can be reduced.
  • the quartz constituting the reaction tube 2 and the like may contain (diffuse) fluorine which can be diffused in the cleaning process (described later).
  • the activated ammonia reacts with the fluorine diffused in the quartz, and the fluorine diffuses from the quartz in the reaction tube 2 (outward diffusion).
  • the amount of fluorine diffused into the quartz constituting the reaction tube 2 is reduced, and the diffusion of fluorine from the reaction tube 2 during the film formation process can be reduced.
  • the amount (concentration) of fluorine in the silicon nitride film formed by the film forming process can be reduced.
  • the surface of quartz constituting the reaction tube 2 and the like is nitrided by the activated ammonia. For this reason, it is difficult for impurities to diffuse outward from the quartz into the reaction tube 2, and it is possible to suppress impurities such as metal contaminants from being mixed into a silicon nitride film formed in a film formation process described later.
  • the surface of quartz constituting the reaction tube 2 and the like is nitrided by using the activated ammonia such as N * and NH * to form a nitride film, impurities such as metal contamination are generated. It is difficult to be released from the quartz into the reaction tube 2. For this reason, it is more preferable to form a nitride film on the surface of quartz constituting the reaction tube 2 and the like with the activated ammonia.
  • the vacuum pump 20 is driven to discharge the gas in the reaction tube 2.
  • a predetermined amount of nitrogen gas is supplied from the purge gas supply pipe 17.
  • the gas in the reaction tube 2 is exhausted to the exhaust tube 18 Will be issued.
  • the temperature inside the reaction tube 2 is adjusted to a predetermined temperature, for example, 300 ° C. as shown in FIG.
  • the pressure in the reaction tube 2 is returned to normal pressure (stabilization step). Then, the lid 7 is lowered by the boat elevator 8 to perform unloading (unloading process).
  • a film forming process for forming a silicon nitride film on the semiconductor wafer 10 is performed.
  • the inside of the reaction tube 2 is heated to a predetermined load temperature, for example, 300 ° C. as shown in FIG.
  • a predetermined load temperature for example, 300 ° C.
  • the lid 7 lowered by the boat elevator 8
  • the wafer boat 9 containing the semiconductor wafer 10 is placed on the lid 7.
  • a predetermined amount of nitrogen gas is supplied from the purge gas supply pipe 17 into the reaction pipe 2.
  • the lid 7 is lifted by the boat elevator 8 to load the wafer boat 9 into the reaction tube 2.
  • the semiconductor wafer 10 is accommodated in the inner tube 3 of the reaction tube 2 and the reaction tube 2 is sealed (loading step).
  • the vacuum pump 20 is driven while controlling the opening of the valve 19 to discharge the gas in the reaction tube 2, and the pressure in the reaction tube 2 is reduced.
  • the discharge of the gas in the reaction tube 2 is continued until the pressure in the reaction tube 2 reaches a predetermined pressure, for example, 26.5 Pa (0.2 Torr) as shown in FIG. 2 (b).
  • the temperature inside the reaction tube 2 is raised to a predetermined temperature, for example, 760 ° C. as shown in FIG.
  • the above-described operation of reducing the pressure and raising the temperature is continued until the reaction tube 2 is stabilized at the predetermined pressure and temperature (stabilization step).
  • a predetermined amount of nitrogen gas is supplied from the purge gas supply pipe 17.
  • the gas in the reaction tube 2 is discharged to the exhaust tube 18 (purge step).
  • the gas discharging process and the nitrogen gas supplying process in the reaction tube 2 are repeated a plurality of times.
  • a predetermined amount of nitrogen gas is supplied from a purge gas supply pipe 17, and the inside of the reaction pipe 2 is returned to normal pressure. Thereafter, the lid 7 is lowered by the boat elevator 8, and the wafer boat 9 (semiconductor wafer 10) is unloaded from the reaction tube 2 (unloading step).
  • Such a film formation process may be repeatedly performed a plurality of times after the purge process is performed. For example, after performing a purging process to clean the heat treatment apparatus 1, the film forming process may be repeated a predetermined number of times.
  • a silicon nitride film can be continuously formed on the semiconductor wafer 10. If the purging process and the film forming process are always performed alternately, it is possible to reduce the contamination of the formed silicon nitride film with metal nitride and fluorine.
  • the amount of metal contamination and fluorine in the quartz constituting the reaction tube 2 can be reduced, and the diffusion of metal contamination and the like from the reaction tube 2 during the film formation process can be reduced. Can be.
  • the contamination of the silicon nitride film formed by the film formation process with impurities can be reduced, and the concentration of the impurities in the silicon nitride film can be reduced.
  • the surface of quartz constituting the reaction tube 2 and the like is nitrided by utilizing radicals such as N * and NH * of the activated ammonia to form a nitride film. It becomes difficult for impurities to be further diffused (outwardly diffused) into the inside. As a result, the incorporation of impurities into the silicon nitride film formed by the film forming process can be reduced, and the concentration of impurities in the silicon nitride film can be reduced.
  • a method for forming a thin film including a cleaning process for removing deposited silicon nitride and a purging process will be described.
  • the cleaning process and the purging process correspond to the cleaning method of the thin film forming apparatus in the present invention.
  • the inside of the reaction tube 2 is heated to a predetermined load temperature, for example, 300 ° C. as shown in FIG.
  • a predetermined load temperature for example, 300 ° C.
  • the wafer boat 9 containing the semiconductor wafers 10 is placed on the lid 7 with the lid 7 lowered by the boat elevator 8.
  • a predetermined amount of nitrogen gas is supplied from the purge gas supply pipe 17 into the reaction pipe 2.
  • the lid 7 is lifted by the boat elevator 8 to load the wafer boat 9 into the reaction tube 2.
  • the semiconductor wafer 10 is accommodated in the inner tube 3 of the reaction tube 2 and the reaction tube 2 is hermetically closed (about a single door).
  • the vacuum pump 20 is driven while controlling the opening of the valve 19 to discharge the gas in the reaction tube 2, and the pressure in the reaction tube 2 is reduced.
  • the discharge of the gas in the reaction tube 2 is continued until the pressure in the reaction tube 2 reaches a predetermined pressure, for example, 26.5 Pa (0.2 Torr) as shown in FIG. 3 (b).
  • the temperature inside the reaction tube 2 is raised to a predetermined temperature, for example, 760 ° C. as shown in FIG.
  • the above-described operation of reducing the pressure and raising the temperature is continued until the reaction tube 2 is stabilized at the predetermined pressure and temperature (stabilization step).
  • the silicon nitride generated during the film forming process is not only treated on the surface of the semiconductor wafer 10 but also on a heat treatment device such as the inner wall of the inner tube 3 (thin film forming device). ) It is also deposited (adhered) inside 1. Therefore, after the film forming process has been performed a predetermined number of times, a cleaning process for removing silicon nitride adhered inside heat treatment apparatus 1 is performed.
  • a cleaning gas containing a fluorine gas (F 2 ), for example, a gas composed of a fluorine gas, a hydrogen fluoride gas (HF), and a nitrogen gas (N 2 ) as a diluting gas is used.
  • F 2 fluorine gas
  • HF hydrogen fluoride gas
  • N 2 nitrogen gas
  • the wafer boat 9 containing no semiconductor wafer 10 is placed on the lid 7. Place. Then, the lid 7 is raised by the boat elevator 8 to seal the reaction tube 2 (loading process).
  • the gas in the reaction tube 2 is discharged, and the inside of the reaction tube 2 is maintained at a predetermined pressure, for example, 2 OOOOPa (150 Torr), as shown in FIG. Further, the inside of the reaction tube 2 is heated (maintained) to a predetermined temperature, for example, 300 ° C. as shown in FIG.
  • a predetermined pressure for example, 2 OOOOPa (150 Torr)
  • the inside of the reaction tube 2 is heated (maintained) to a predetermined temperature, for example, 300 ° C. as shown in FIG.
  • stabilization step The above-described operation of reducing the pressure and raising the temperature is continued until the reaction tube 2 is stabilized at the predetermined pressure and temperature (stabilization step).
  • a predetermined amount of a cleaning gas for example, 2 liters of fluorine gas Zmin as shown in FIG. 3 (f) and a gas shown in FIG. As shown in FIG. 3 (c), 2 l / min of hydrogen fluoride gas and 8 l / min of nitrogen gas were introduced into the inner tube 3. Is entered.
  • the introduced cleaning gas is heated in the inner pipe 3 and discharged from the inner pipe 3 to the exhaust pipe 18 through a space formed between the inner pipe 3 and the outer pipe 4.
  • the cleaning gas comes into contact with the silicon nitride adhering to the inner wall and the outer wall of the inner pipe 3, the inner wall of the outer pipe 4, the inner wall of the exhaust pipe 18, the inner surface of the heat treatment apparatus 1 such as the boat 9, and the like. Is etched. Thereby, the silicon nitride adhered to the inner surface of the heat treatment apparatus 1 is removed (cleaning step).
  • a fluorine gas when supplied into the reaction tube 2 in the cleaning step, for example, fluorine diffuses into quartz constituting the reaction tube 2.
  • the fluorine is diffused (outwardly diffused) from the reaction tube 2 during the film formation process, and is formed on the semiconductor wafer 10, for example.
  • the concentration of fluorine in the silicon nitride film increases.
  • a fluorine-based impurity for example, SiF
  • the supply of the cleaning gas from the cleaning gas introduction pipe 14 is stopped.
  • a predetermined amount of nitrogen gas is supplied into the reaction tube 2 from the purge gas supply tube 17, and the gas in the reaction tube 2 is discharged.
  • the inside of the reaction tube 2 is set to a predetermined pressure, for example, the above-mentioned 133 Pa (1.0 Torr) to 53.3 kPa (400 Torr). In the present embodiment, as shown in FIG. 3B, the pressure is set to 2660 Pa (20 Torr).
  • the inside of the reaction tube 2 is set to a predetermined temperature, for example, the above-mentioned 600 ° C. to 1050 ° C. by the heater 12 for raising the temperature.
  • the temperature is raised to 900 ° C. as shown in FIG.
  • the above-described operation of reducing the pressure and raising the temperature is continued until the reaction tube 2 is stabilized at a predetermined pressure and temperature (a stabilization step).
  • a predetermined amount of nitrogen-based gas for example, ammonia gas as shown in FIG. L / min supplied.
  • the vacuum pump 20 is driven while the opening of the valve 19 is controlled, and the gas in the reaction tube 2 is discharged.
  • the supply of the ammonia gas and the discharge of the gas in the reaction tube 2 are repeated a plurality of times. (Ammonia purge step).
  • the ammonia in the reaction tube 2 is excited (activated) by the heat in the reaction tube 2.
  • the ammonia easily reacts with the fluorine diffused in the stones constituting the reaction tube 2 to generate, for example, ammonium fluoride (NH 4 F).
  • NH 4 F ammonium fluoride
  • fluorine is discharged out of the reaction tube 2.
  • the amount of fluorine diffused into the quartz constituting the reaction tube 2 is reduced, and the diffusion of fluorine from the reaction tube 2 during the film forming process can be reduced.
  • the fluorine concentration in the silicon nitride film formed by the film forming process can be reduced.
  • the activated ammonia can also react with metal contamination contained in quartz constituting the reaction tube 2.
  • metal contamination is diffused (outwardly diffused) from inside the quartz of the reaction tube 2 and becomes chewy.
  • metal contamination contained in the quartz constituting the reaction tube 2 is reduced, and diffusion of the metal contamination from the reaction tube 2 during the film forming process can be reduced.
  • the amount (concentration) of metal contamination in the silicon nitride film formed by the film forming process can be reduced.
  • the activated ammonia causes the surface of the quartz constituting the reaction tube 2 to be nitrided. For this reason, the fluorine in the quartz hardly diffuses from the reaction tube 2, and the diffusion of the fluorine from the reaction tube 2 during the film forming process can be reduced. As a result, the concentration of fluorine in the silicon nitride film formed by the film forming process can be reduced. Further, it is possible to prevent impurities from being mixed into the silicon nitride film. In particular, when the surface of the quartz constituting the reaction tube 2 and the like is nitrided by utilizing radicals of activated ammonia such as N * and NH *, a nitride film is formed. It is difficult for impurities to diffuse into the inside. For this reason, it is more preferable to form a nitride film on the surface of quartz constituting the reaction tube 2 and the like with activated ammonia.
  • the vacuum pump 20 is driven to discharge the gas in the reaction tube 2.
  • a predetermined amount of nitrogen gas is supplied from the purge gas supply pipe 17.
  • the gas in the reaction tube 2 is discharged to the exhaust pipe 18.
  • the temperature inside the reaction tube 2 is increased to a predetermined temperature, for example, as shown in FIG. Adjusted to 0 ° C.
  • the pressure in the reaction tube 2 is returned to normal pressure (stabilization step).
  • the lid 7 is lowered by the boat elevator 8 and unloading is performed (about 1 door).
  • the silicon nitride film can be continuously formed on the semiconductor wafer 10 by repeating the cleaning method of the thin film forming apparatus including the cleaning process and the purge process after the predetermined number of film forming processes. .
  • a cleaning process and a purge process may be performed after each film forming process.
  • the inside of the furnace (the inside of the reaction tube 2) is cleaned every time, and the contamination of the metal nitride and the fluorine into the formed silicon nitride film can be reduced.
  • the amount of fluorine diffused into the quartz constituting the reaction tube 2 by the cleaning process can be reduced, and the diffusion of fluorine and the like from the reaction tube 2 during the film formation process can be reduced. 'Can be reduced. Therefore, the concentration of fluorine in the silicon nitride film formed by the film forming process can be reduced. It is also possible to prevent fluorine-based impurities such as SiF from being mixed into the silicon nitride film. That is, the incorporation of impurities into the silicon nitride film formed by the film formation process can be reduced, and the concentration of impurities in the silicon nitride film can be reduced.
  • the reaction tube 2 and the like is nitrided by utilizing radicals of activated ammonia such as N * and NH * to form a nitride film
  • the reaction tube is removed from the quartz. It becomes difficult for impurities to be further diffused (outwardly diffused) into the inside. As a result, contamination of impurities into the silicon nitride film formed by the film formation process can be reduced, and the concentration of impurities in the silicon nitride film can be reduced.
  • the quartz chip was housed in the heat treatment apparatus 1 (reaction tube '2), and was subjected to a cleaning process using a cleaning gas containing fluorine gas.
  • the quartz chip The fluorine concentration in the depth direction is measured. Was decided.
  • the secondary ion intensity of nitrogen was measured by secondary ion mass spectrometry (SIMS).
  • FIG. 4 shows the relationship between the depth of the quartz chip and the fluorine concentration.
  • Figure 5 shows the relationship between the depth of the quartz chip and the secondary ion intensity of nitrogen.
  • the secondary ion intensity of nitrogen was improved by performing the ammonia purge.
  • the secondary ion intensity of nitrogen greatly improved. That is, the vicinity of the surface of the quartz chip is nitrided by the ammonia purge.
  • a conventional nitrogen purge (N 2 purge) using a nitrogen gas or an ammonia gas of the present invention is used.
  • the wafer is placed in the reaction tube 2 that has been purged with ammonia (NH 3 purge), and the wafer is heated by raising the temperature of the reaction tube 2 to 800 ° C, and then heated.
  • the wafer was taken out and the copper concentration on the wafer surface was measured.
  • Figure 6 shows the results. As shown in FIG. 6, the copper concentration was measured at predetermined five points in the wafer surface by the total reflection X-ray fluorescence method.
  • the temperature inside the reaction tube 2 was set at 950 ° C. and the pressure was set at 159 Pa (120 Torr). Ammonia gas was supplied into 2 at 2 liters Zmin.
  • the amount of fluorine and metal contaminants in the reaction tube 2 is reduced by the ammonia purge, so that the amount of fluorine and metal contamination from the reaction tube 2 during the film forming process is reduced. Diffusion can be reduced. As a result, it is possible to reduce the fluorine concentration in the silicon nitride film formed by the film forming process. Further, it is possible to prevent impurities such as metal contaminants from being mixed into the silicon nitride film. Further, according to the present embodiment, since the surface of the stone constituting the reaction tube 2 is nitrided by the ammonia purge, it is possible to reduce the diffusion of fluorine and metal contamination from the reaction tube 2 during the film forming process. it can. As a result, the concentration of fluorine in the silicon nitride film formed by the film forming process can be reduced. In addition, it is possible to prevent impurities such as metal contamination from being mixed into the silicon nitride film.
  • the nitrogen-based gas that has not been activated is supplied into the reaction tube 2 heated to a predetermined temperature (900 ° C.) and activated.
  • an activating means 31 may be provided in the nitrogen-based gas introduction pipe 15 to supply the activated nitrogen-based gas into the reaction pipe 2.
  • the activating means 31 includes a heating means, a plasma generating means, a photolytic means, a catalyst activating means and the like.
  • ammonia is used as the nitrogen-based gas.
  • the nitrogen-based gas may be any gas containing nitrogen and being activatable, for example, nitrous oxide or nitric oxide.
  • the cleaning gas may be any gas containing fluorine, for example, fluorine and chlorine such as C 1 F 3. Gas may be used.
  • the reaction tube 2 and the like are formed of quartz.
  • the material from which the reaction tube 2 and the like are formed is not limited to quartz.
  • the present invention is effective for a material in which fluorine diffuses, such as a SiC material.
  • a material having excellent heat resistance is preferable.
  • the silicon nitride film is formed on the semiconductor wafer 10.
  • the present invention is also effective for a thin film forming apparatus for forming a titanium nitride film on a semiconductor wafer 10, for example.
  • the temperature inside the reaction tube 2 is set at 900 ° C. and the pressure is set at 266 Pa (20 Torr), and the ammonia purge is performed.
  • the temperature and pressure in the reaction tube 2 are not limited to these.
  • the temperature inside the reaction tube 2 may be set to 950 ° C., and the pressure may be set to 159 Pa (120 Torr).
  • the quartz surface of the reaction tube 2 is further nitrided, and the diffusion of fluorine and the like from the reaction tube 2 during the film forming process can be further suppressed.
  • the frequency of cleaning may be performed every several film formation processes or may be performed every single film formation process.
  • the batch type vertical heat treatment apparatus having the double tube structure in which the reaction tube 2 includes the inner tube 3 and the outer tube 4 has been described, but the present invention is not limited to this.
  • the present invention can be applied to a batch type heat treatment apparatus having a single pipe structure without the inner pipe 3.
  • the object to be processed is not limited to the semiconductor wafer 10, but may be applied to, for example, a glass substrate for LCD.

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Abstract

L'invention concerne un procédé permettant de nettoyer un appareil de formation de films minces, selon lequel un film mince est formé sur un objet à traiter, par apport d'un gaz de traitement dans une chambre de réaction où l'objet se trouve. Ledit procédé de nettoyage comprend une étape de purge pour purger l'intérieur de la chambre de réaction, par introduction d'un gaz azoté activable contenant de l'azote dans la chambre de réaction. Cette étape de purge comprend une sous-étape au cours de laquelle le gaz azoté est activé pour nitrurer les surfaces d'éléments situés dans la chambre de réaction.
PCT/JP2004/004205 2003-03-25 2004-03-25 Procede de nettoyage d'un appareil de formation de films minces WO2004086482A1 (fr)

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JP4430918B2 (ja) 2010-03-10
KR100779823B1 (ko) 2007-11-28
TWI336492B (fr) 2011-01-21
US20060213539A1 (en) 2006-09-28

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